Water → HCID 70533310, Verbindung

HRID 435449Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435449
[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10](O)[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=S(Cl)[Cl:26].C(Cl)Cl.O>CCOCC.N1C=CC=CC=1>[C:1]1([C:7]2[C:8]3[O:13][CH2:12][O:11][CH:10]([Cl:26])[C:9]=3[CH:15]=[CH:16][C:17]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 6344DichloromethaneHCID 24386Thionyl ChlorideHCID 70532672HCID 70532672, Verbindung

Produkt 1

HCID 70533310HCID 70533310, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 3283Diethyl EtherLösungsmittel2×

Versuchsvorschrift

To a stirred solution of 11.6 g. (38 mmol) of 3,4-diphenylmethylenedioxybenzyl alcohol in ether (80 ml.) and pyridine (0.6 ml.) at 20° C. was added dropwise a solution of SOCl2 in ether (40 ml.). The mixture was cooled to 0°-5° C., and CH2Cl2 and water were added. The layers were separated, and the organic layer was washed with water and saturated aqueous NaCl, dried over MgSO4 and concentrated to dryness to yield 3,4-diphenylmethylenedioxybenzyl chloride (11.43 g.) as a colorless viscous oil: tlc (silica gel CH2Cl2 : Rf 0.8; ir (CCl4) no --OH--, nmr (CCl4) δ 4.34 (s, 2H), 6.74 (d,j=8) 2H, 6.67 (s, 1H), 7.1-7.6 (m, 10H). ##STR11##

Aufarbeitung

  1. temperatureThe mixture was cooled to 0°-5° C.
  2. customThe layers were separated
  3. washthe organic layer was washed with water and saturated aqueous NaCl
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-184d5f6240034e1bb527e37469b92536
Quelldatensatz
uspto-grants-1983_08
Patentnummer
US04401676

Notizen zur Reaktion

Wird geladen…